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To a suspension of 2-(1 ,2-benzisoxazol-3-yl)acetic acid (0.4951 g, 1 eq) inDCM (15 ml), 1 -ethyl-3-(3-dimethylaminopropyl)carbodiimide (0.6429 g, 1 .2 eq) and A- dimethylaminopyridine (0.4097 g, 1 .2 eq) are added. The resulting brown solution is5 stirred for 10 min and trifluoromethanesulfonamide (0.5 g, 1 .2 eq) is then added. The reaction mixture is stirred at room temperature overnight, diluted with DCM, washed with 5% KHSO4 and water, dried over MgSO4 and evaporated to dryness, to give a yellowish solid. This crude material is purified by preparative HPLC, to afford a white powder (0.1 10 g, 13% yield). LC-ESI-HRMS of [M+H]+ shows 309.0156 Da. CaIc.10 309.015688 Da, dev. -0.3 ppm.
Add 50 ml of deionized water, 0.01 mol of trifluoromethanesulfonamide, 0.01 mol of potassium hydroxide, and 0.01 mol of potassium carbonate in a 250 ml three-necked flask, and mix well; after the temperature returns to room temperature, add 0.0005 mol of diaminopyridine, stir and dissolve, and then drop. 50 ml of a chloroform solution in which 0.01 mol of 5-iodo-3-oxa-octafluoropentylsulfonyl fluoride was dissolved, and reacted at 1000 rpm with stirring0.5h. The reaction product was separated into an aqueous phase, the pH was adjusted to 4 with 5% hydrochloric acid, and ethyl acetate was evaporated.The yield was about 88%.
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